Lubricants for textile materials



Patented Nov. 30, 1948 LUBRICANTS FOR TEXTILE MATERIALS AbrahamMoscowitz, New York, N. Y., assignor to L. Sonneborn Sons, line., acorporation of Delaware No Drawing. Application November21, 1946,

Serial No. 711,475

6 Claims. i

This invention relates to new and useful improvements in lubricants fortextile materials.

In textile processing such as of wool. worsted, rayon, viscose or thelike, the raw materials are converted to fibres, the fibres formed intothreads, the threads woven into fabric and the woven fabric furtherprocessed and finally dyed.

In the processing of wool or worsted, or the like, the raw material suchas raw wool is subjected in pickers to an opening operation, 1. e.,freeing of the fibres as much as possible with a minimum of breakage.Thereafter the fibres are carded, i. e., fully opened and subjected to aroving operation, 1. e., the formation of a continuous form of fibre orroving prior to spinning. The roving is spun into threads and thethreads woven into fabric, the woven fabric being then fulled andfinally dyed. These operations, up to the fulling step, including avariety of intermediate steps not herein enumerated, require thepresence of a lubricating agent. This agent is conventionally added inthe pickers prior to carding and may be applied either straight or inthe form of emulsions. The'latter is the more common procedure; theemulsion usually contains about 25% of the composition and isconventionally applied as a spray. The wool is impregnated to retainabout to of the composition. Normally the conditions of processing aresuch that the water of the applied emulsion largely evaporates by thetime the impregnated material is spun, the material ordinarily reachingthis stage with a desired water content which may range for example from5 to the preferred water content being inter alia dependent upon thetype of material processed. The fulling step as such involves amechanical beating of the fabric in drip-wet condition in the presenceof a fulling agent and serves to densify the material, giving it itscharacter, construction and appearance. or of the alkaline type.Alkaline fulling agents are the more common and usually comprise about 6to 8% soap. Two to four percent of soda are also conventionally added asan aid to the action of the fulling agent. The drip-wetness of thefabric in the fulling step is usually defined by a water content ofbetween 80 and 100% and sometimes higher of water per dry weight ofgoods.

In conventional practices the lubricant on the fibre, such as wool, whenreaching the fulling step is antagonistic to the fulling operation andlargely prevents the necessary wetting contact of the water with thefibre. It is inter alia for this reason that such relatively largeamounts of fulling agents have to be added, 1. e., to counteract thisaction of the lubricant.

In the processing of synthetic materials such as rayon, viscose or thelike, filaments as they come from the spinning solution or bath areconverted into yarn and the yarn knitted or woven Fulling agents may beeither of the acid into fabric. The formation of the yarn prior to theweaving includes such processing steps as coning, quilling and combing,all of which, together with the subsequent weaving or knitting, alsonecessitate theme of a suitable lubricant. Such lubricant isconventionally the same composition or of the same type as that used inwool processing and is normally applied to the loosely held togetherfilament cakes either as such, i. e., straight, or in the form ofaqueous emulsions. When the textile lubricant composition is applied byway of emulsion, usually a 1 to 4% aqueous emulsion is employedand-penetrates the filament cake leaving on the fibre approximately to2% of the lubricant which in the majority of cases is satisfactory forthe intended purpose. The lubricant at the same time acts as a softeningagent. Once the filaments are converted into yarn, the yarn is firstused for the setting of warp threads as the first step in the weavingoperation. These warp threads are then first sized with a suitable sizesolution, such as gelatin or the like, to condition them for thesubsequent weaving operation. Conventional textile lubricant impregnantsare antagonistic to the size solution and it is necessary to incorporatea wetting agent in the size to overcome the repelling effect of theimpregnant.

The hitherto used textile lubricants are also antagonistic to the dyeingoperation of both wool type and synthetic type fibres in that theyinterfere with the requisite wetting contact between the dye bath andthe fibre and must be removed therefore prior to the dyeing step. Thisremoval is carried out in a scouring operation in which the goods areexhaustively washed with water containing scouring agents, such assoaps, usually in the presence of alkalis, such as soda ash. The use ofthe securing agents, however, does not efiectuate the substantiallycomplete removal of the conventional lubricating compositions from thefibres of the fabric treated. Substantial complete removal of lubricantas generally understood in the art is defined as 85-90% or betterremoval (plant run test) of the lubricant used. In the majority of casesscourability of lubricating agents used in conventional practicesnormally results in lubricant removal of not better than about -77% byplant run test which is equivalent to about 60 to by laboratory test, i.e., as determined by conventional laboratory scourability tests. (Plantrun scourability values are usually about 10% higher than the valuesindicated by laboratory scourabllity tests.) By reason therefore of thisinsuflicient scourability of the conventional impregnants appreciableamounts of lubricant are carried over into the dyeing bath and therenecessitate the use of dyeing assistants. The use of soaps and/oralkalis in securing operations often exercises a detrimental effect uponthe fibres and/or fabric- One object ofthe invention comprises interalia a lubricant for textile materials substantially tree from theaforementioned defects inherent in conventional textile treatingcompositions, and which, when carried as impregnant on a textilematerial substantially eliminates the aforesaid drawbacks anddisadvantages of conventional practices or products in the processing oftextile materials.

The foregoing and further objects of the invention will be apparent fromthe following description.

When treating a petroleum distillate stock with fuming sulfuric acidunder sulfonating conditions of acid amount and temperature inaccordance with conventional refining practice, an oil layer and acidsludge layer are formed. The oil layer contains dissolved thereinpetroleum sulfonic acids, collectively referred to as mahogany petroleumsulfonic acids, which are recovered therefrom in accordance withconventional methods in the form of solutions of these sulfonic acids ortheir salts (herein collectively termed "petroleum mahogany sulionates)in a portion of the oil relatively tenaciously occluded by thesesulfonic bodies and generally referred to in the art as retained oil.These petroleum sulfonic acids or suli'onate oil compositions normallycontain about 30 to 35% of retained oil and 65 to 70% of the petroleummahogany sulfonic material. Depending upon the type and origin ofpetroleum oil distillates from which these sulionate-oil solutions orstocks are derived they contain sulionates of varying averaged molecularI weights. For convenience therefore the sulfonate stocks are identifiedby their averaged molecular weights. Thus a. 4.20 or 450 sulfonate stockis a stock in which the sulionates have an average molecular weight of420 or 450 respectively.

Petroleum mahogany sulfonate solutions are extremely viscous incharacter even when reduced by the addition oi further amounts of oil toas low as 20% sulfonate content, and are, as such, unsuitable for use astextile lubricants since it is a prerequisite for textile lubricationthat the impregnating material does not normally exceed a viscosity of600 seconds Saybolt at 100 F. This is by reason of the fact that higherthan 600 seconds Saybolt viscosities will not flow sufliciently freelyfor satisfactory impregnation and will tend to such relative stickinessas to seriously impair their lubricating properties. Thinning withnonlubricating solvents is normally not successful as these will eitherevaporate, thus leaving behind a viscous, sticky impregnating materialwithout adequate lubricating capacity'on' the fibre, or will interferewith the. scouring operation. on the other hand, thinning with a textilelubricant type diluent will not obtain the desired result, as it isnecessary to add so much of the diluent as to bring the sulfonatecontent to below that necessary for adequate emulsiflcation or evenminimumconventional scourability. Even disregarding the viscositylimitation the highest heretofore proposed amounts of 25% sulfonatecontent (Reddish U. 8. 1,909,721, Twitchell U. 8. 1,794,342) fall toimpart substantial seli-scourability.

In accordance with the invention the normally high viscosity of analkali metal petroleum mahogany sulfonate solution in a textilelubricant hydrocarbon can be reduced to a point permitting the obtainingof-such solution with a viscosity not exceeding 600 seconds Sayboltatl00 F. and containing in excess of 28% sulfonates, and theimpregnation of a textile material, prior to spinning or otherfabrication into yarn, with lubricating amounts of suchviscosity-reduced solution yields a substantially selbscouringlubricated textile product ready for further processing. If theimpregnated textile material is wool a substantially self-tulling aswellas self-scouring lubricated wool is obtained. This impregnated woolpermits a simplified processing in which it is subjected to a fullingoperation with water in substantially drip-wet amounts and substantiallyfree from fulllng agents. The process may additionally include, afteriulling, a scouring operation with substantially exhaustive amounts ofwater substantially free from scouring agents followed by dyeing, or, adyeing operation without prior scouring, i. e., with the .impregnantsubstantially remaining in or on the wool when the same enters the dyebath. Thus in the case of wool the lubricating impregnant is per seiulling agent and also a dyeing assistant.

The aforementioned viscosity reduction is preferably carried out bysubjecting the petroleum mahogany sulfonate textile lubricanthydrocarbon solution, containing in excess of 28% sulfonate and havingby reason of the sulionate content a viscosity in excess of 600 secondsSaybolt at F., to a viscosity reducing reaction. The viscosity reducingreaction may be an oxidation reaction, 1. e., a reaction in which anoxidation potential exists. The oxidation reaction may be induced bymaterials in which the oxidation potential exists by virtue of thepresence or liberation of 02, such materials including inorganicoxidation agents such as chromic acid, bichromates, peroxides, etc., aswell as organic oxidation agents and particularly organic peroxides suchas benzoylperoxide, butylperoxide and similar materials. The oxidationreaction may be induced by materials in which the oxidation potentialexists by reason of the presence of what is conventionally termed"active chlorine as it is present in oxidatively acting chlorine,chlorine oxides, such as C and C102, or oxldatively acting derivatives,both inorganic and organic, of the various chlorine-oxygen acids ortheir salts as for example hypochlorous acid (HOCl), hypochlorites,organic hypochlorous derivatives including those of the chloramine typesuch as toluene sulfonchloramide and benzene sulionchloramide, chlorousacid (HClOz), chlorites, as well as combinations of these activechlorine containing agents. Alternatively, the viscosity reducingreaction may be obtained by treatment with relatively small amounts ofsuch agents as various diethylene glycol esters and phthalic acid estersand particularly dimethyl phthalate.

The reaction conditions under which the oxidizing substances produce anoxidation potential are well known in the art and need not befurtherexernplifled here except with respect to the preferred proceduresfor the procurement of a hypochlorite at a pI-Irange of about 6-8 andpreferably at a neutral to alkaline pH, or, with alkali metal chloriteat an acid pH. Thus for instance the hydrocarbon solvent solution of asuitable mahogany sulfonate may be subjected to a hypochlorite treatmentsubstantially as set forth in the Blumer et a1 U. S. Pat. 2,201,119using amounts of hypochlorite sumcient to obtain the desired viscosityreduction which is accompanied by the color reduction to a Lovibondvalue of less than 8R white oil solution V2" cell) as set forth in saidpatent. Alternatively, such solution may be intimately contacted with asuitable chlorite at a pH below 7 in accordance with the procedure setforth in the Liberthson et a1. patent, U.S. 2,307,743, using amounts ofchlorlte sufficient to obtain the desired viscosity reduction which isaccompanied by the color reduction to a Lovibond value of less than8R-(10% white oil solution cell) as set forth in said patent.

For best results, however, a combination of the chlorite andhypochlorite treatment is preferred. In the preferred mode of suchtreatment, 1.5-7 and preferably 2.5-6% of the chlorite and hypochlorite(calculated in the aggregate dry weight by weight of sulfonate insolution) are used in a proportion of 0.5 to 4 parts by weight andpreferably of 2 to 3 parts by weight of hypochlorite for every one partby weight of chlorite. The v'iscosity reduction reaction is carried outwith this procedure by intimately contacting the chlorite hypochloritecombination with the sulfonate hydrocarbon solution until the desiredviscosity reduction is obtained. The pH of reaction may be on thealkaline or acid side avoiding an excess on either side. When operatingon the acid side neutralization is necessary. This is usuallyaccompanied by some increase in viscosity of the reaction reducedviscosity. For this reason it is of advantage to select the pH ofreaction at 7 or higher and preferably at from 7.5-8.5; if necessary thesolution may be acidified with H2504 to that range. The preferred modeof operation is to dissolve the chlorite in the aqueous hypochloritesolution. The temperature is ordinarily not critical. The reactionhowever may be facilitated by increasing the temperature to for examplea preferred temperature. of from 120 to 200 F.; this will increase thefluidity of the petroleum hydrocarbon, thus permitting more intimatecontact between the reactants. The combination chlorite-hypochlorite.treatment within the preferred scope of my invention effectuates alarger viscosity reduction with a lesser amount of total chlorineoxidation reagents than is the case with either the chlorite orhypochlorite treatment alone.

The viscosity reducing reaction is carried out as stated on a textilelubricant hydrocarbon soa textile lubricant hydrocarbon solutioncontaining relatively high concentrations of petro leum mahoganysulfonate, as for instance in excess of 40% petroleum mahoganysulfonate, in which case the resultant product is a concentrate whichmust then be adjusted by the addition of textile lubricant hydrocarbonof suitable viscosity to the requisite petroleum mahogany sulfonatecontent, 1. e., in excess of 28% and preferably between 28 and 40% and aviscosity below 600 and preferably for wool below 500 and for syntheticfibre below 300 seconds Saybolt at 100 F. Generally solvent extension toreduce viscosity of a treated concentrate to below 600 seconds Sayboltat 100 F. will simultaneously bring the sulfonate content to 40% orlower. The viscosity of the extending hydrocarbon lubricant should be soselected that the viscosity of the finished product is maintained belowits desired top limit. In the viscosity reducing reaction, inorganicsalts are formed which if produced in excessive amounts may sumcientlyinterfere with the emulsifying or wetting or re-wetting properties ofthe resultant product to make their removal in the conventional manneradvisable. In

many cases however such relatively small quanlution of in excess of 28%alkali metal petroleumv mahogany sulfonate content, which solutionpossesses normally a viscosity in excess of 600 secsufficiently large tomaterially impair the desirable textile processing properties of theimpregnant. These can then be carried into the finished product withoutnecessity for removal.

When proceeding in accordance with the invention it is in most cases ofadvantage to use the sulfonate product obtained in the conventional acidrefining petroleum oil distillates andcontaining about 61-2% petroleummahogany sulfonates (having an average molecular weight for example offrom 400-550) and about 37-8% retained 011. Such a product may normallypossess, for instance, a viscosity of about 80 to 205 furol at 210 F.and, after treatment with,

for instance, the chlorite hypochlorite combination, a reduced viscosityof between 38 and 112 furol at 210 F. which when diluted with ahydrocarbon and preferably a mineral oil stock of suitable viscositysuch as 75 seconds Saybolt. at 100 F. to a 30% sulfonate content yieldsa viscosity of about 370 to 380 seconds Saybolt at 100 F.

Alternatively, t e novel impregn'ant may be ob-' tained directly assuch,i. e., without necessity for adjustment with extending amounts ofhydrocarbon oii, by a modification of the conventional acid refiningprocedure. When proceeding in this manner a. petroleum oil distillate(containing about 30-35% sulfonatables). is given at a temperature ofabout 150 F. a 50% batch treatment with fuming sulfuric acid, 1. e., atreatment (sometimes in several batches) with 50% of acid by weight ofthe oil treated. The cooled acidified oil is thereafter diluted with anequal volume of benzol, the mixture is permitted to settle overnight andthe acid sludge layer is withdrawn. After neutralizing the oil layer andremoving the benzol by distillation, the oil layer is subjected to asuitable viscosity reducing reaction in accordance with the inventionand preferably any of the herein' described chlorine oxidationreactions.

The resulting products contain approximately 70% of textile lubricantmineral oil and 30% of petroleum mahogany sulfonates and substantiallypossess a viscosity below 600 seconds Saybolt at The expression textilelubricant hydrocarbon" or such similar term as used herein is intendedto 7 designate a hydrocarbon or a hydrocarbon mixture such as a mineraloil or petroleum hydrocarbon oil, as it is conventionally used fortextile lubricating purposes and having normally a minimum viscosity ofabout 40-50 seconds Saybolt at- 100 F.; the maximum viscosity of thehydrocarbon or hydrocarbon mixture is limited in accordance with theinvention so as not to bring the viscosity of the final compositionabove 600 and preferably 300 seconds Saybolt at 100 F. and in most casesthe practical upper viscosity for the lubricant hydrocarbon within the600 seconds limit is about 150 seconds Saybolt at 100 F. and within the300 seconds" limit about 65 seconds Saybolt at 100 F.

Wherever reference is made herein to the expression lubricating amounts"in connection with my new lubricating impregnant on a textile materialin accordance with the invention or where such similar term is used itis intended to designate thereby the amount of lubricant conventionallycarried or required to be carried by a textile material for adequatelubrication in the processing thereof and which, for example, in thecase of wool, worsted or similar materials may average about 2 to 10%lubricant on the fibre and in the case of a synthetic material such asviscose, rayon or the like may average about 0.25 to 2% lubricant on thefibre.

The novel lubricant composition when carried by the material, promotesrather than repels the contact-wetting of the fibre with water. For thisreason, therewith impregnated wool is essentially self-fulling while atherewith impregnated synthetic fibre is essentially self-wetting withrespect to a size solution.

In wool fulling it is desirable for best results to operate at aslightly alkaline pH and to this end small amounts of soda, up to forexample 2% (by weight of the fuliing water) may be added to 40 furtherfacilitate the fulling action of the impregnant. Other than this,however, no soap and no amounts in excess of 2% of soda ash arerequired.

The composition carried by the fabric in accordance with the inventionnot only acts as a fulling agent but continues during the fullingoperation its lubricating function, thus resulting in more efficientfuiling and production of an improved material. In eifect therefore theinstant invention permits the functional carrying of the lubricant fromthe dry part of the wool processing into the wet part of the woolprocessing operation. In the case of conventional wool lubricants, thelubricant function of the material ceases at the end of the dry part ofthe procedure and is carried over into the wet part withoutsubstantially there exercising any beneficial function, being in factdetrimental to the wet-processing steps.

Thus, as above pointed out, when proceeding in accordance with theinvention as applied to wool there is obtained a lubricant impregnatedwool at the beginning of the textile processing operation, in which theimpregnant as such is an efficient lubricating and fulling agent,eliminating the necessity for the otherwise costly and cumbersomeconventional steps of adding a fulling, agent in the fulling operationand a scouring agent in the scouring operation. The lubricantimpregnated wool fabric in accordance with the invention emerges fromthe water scour with at least 90% (plant run test) of the impregnatingagent removed. The lubricant on the wool constitutes in itself a dyeingaid and permits the 75 direct dyeing of the wool, after fulling, withouta prior scour. In the latter case, it is recommended, however, that theimpregnated material be given a light rinse after fulling, so as tosubstantially remove any pH. controlling agents, as for example smallamounts of soda ash, that may have been used in the fulling and whichmay be harmful to the dyeing or the shades of the dyed material. Some ofthe lubricant is removed with the rinse. All lubricant on the fibre whenit enters the dye bath is effectively removed by the aqueous dyeingmedium during the dyeing operation. The novel lubricant actuallyimproves the dyeing characteristics of wool impregnated therewith and isnot adeterrent to satisfactory dyeing, such as are conventional typecompositions. By this procedure of using the lubricant composition inaccordance with the invention as a fulling aid, a hand of material farsuperior to that obtained from products processed in the conventionalmanner is obtained.

My novel lubricant impregnant as it is present on the fibre andcontaining in excess of 28% sulfonate is substantially spontaneouslydispersed, when contacted by water, in a manner assuring such finenessof dispersed globules of lubricant in the water of contact that thedispersion is of a magnitude approaching true solution, 1. e., themajority of the dispersed globules are in the average of a magnitude ofsize below that of the average wave length of normal light, resulting inthe formation of dispersions that are substantially translucent and forpractical purposes transparent, and thus essentially approach truesolutions. Thus the lubricant impregnants used in accordance with theinvention are not only highly wettable, i. e., emulsiflable ab initio,but are also truly rewettable or reversible, after application to thefibre. They are substantially unaffected by any surface activity of orwithin the fibre and are substantially to the same extent re-'-emulsiflable upon water contact as they originally were when not on thefibre. In the fulling operation of for example wool, at least part ofthe novel impregnant is emulsified. Since only drip-wet amounts of waterare used however in fulling, the impregnant is substantially retained inor on the wool during the physical working of the fulling operation. Atthe same time the pH controlling agent, preferably used when fulling inaccordance with the invention, as for example soda, exercises a somewhatdeterrent effect upon the emulsification of the impregnant and reducesthe capacity of the fulling water for the amount of impregnant which itis able to emulsify. Ordinary viscosity 'unreduced textile lubricanthydrocarbon impregnant compositions, are restricted to a maximum ofabout 15-20% sulfonate content in order not to exceed the maximum usableviscosity limit and do not so react when on the fibre. These, and evencompositions containing as high as 25% sulfonates, when contacted bywater, produce ordinary opaque, milky-emulsion type dispersions, inwhich the particle size of dispersed globules is in the average abovethat of the average wave length of normal light. The surface activity ofthe fibre brings then into play forces of differential adsorption withrespect to these type globules resulting in a relatively tenaciousretention of at least a portion of the lubricant composition. This isone factor in the unsatisfactory scourability of a to)!- tile materialimpregnated with a conventional type mineral oil composition.

The following examples are furnished by way of illustration and not oflimitation:

I 106 lbsz'of a 450 I 1 stock containing 61-2%.mahogany sulionates and Y1 37-38% retained oil was used. 7 The stock was obltia'ar nple petroleummahogany sulfonate tained'from a Mid-Continent stock subjected to 10lbs. of an approxicontainin g 61-2% sodium sulfonates) were heated 1white oil refiningwithfuming sulfuric .acid under sulfonatingconditions;

mately 10% aqueous sodium hypochlorite solution (about 10% available 01)were added to. the mahogany [sulfonate stock. and the mixture wasthereupon agitated, being kept at a. temperatuh of between 200 and 220F.

to 120 F.; a solution of 1 lb. sodium chlorite'in lbs. aqueoushypochlorite solution having a v available chlorine content was added.The'mixture was heated to 200 F. and maintained at this temperature,while. stirring, for one-half hour,

then blown with air to drive out retained moisture and diluted with 75viscosity mineral oil to a 30% suifonate content. Before treatment, thepetroleum sulfonate-retained oil stock had 'a viscos'ity of 163 i'urolat 210 F. and upon dilution to the aqueous hypochlorite solutionevaporated during the treatment. Before treatment the petroleumsulfonate stock had a viscosity of 144 furol at 210 F. and upon dilutionwith amineral pale oil (75 seconds Saybolt at 100 F.) to a sulfonatecontent, a viscosity of 1100 seconds Saybolt at 100 F. vAfter treatmentand before dilution the corresponding viscosity was '74 furol at 210 F.and after dilution with the same 75 viscosity pale oil, 395 secondsSaybolt at 100 F.

Example II 100 lbs. of the same 450 petroleum mahogany sulfonate stockas specified in Example I was adjusted to a pH of 6 to 6.5 and thenabout 3 lbs. of

sodium chlorite was added in the form of a concentrated aqueoussolution. The mix was agitated, maintaining the temperature at aboutbetween 180 and 200 F. Samples were taken at frequent intervals and thetreatment discontinued when a color reduction to about 2-3R (Lovibond10% white oil solution cell) was observed. This result was achievedafter about one-half hour. After treatment the reduced viscosity was 72furol at 210 F. and after dilution with the same 75 viscosity pale oilspecified in Example I, 400 seconds Saybolt at 100 F.

Example III 100 lbs. of petroleum sulfonate-retained oil stock 30%sulfonate content 1463 Saybolt at 100. After treatment and beforedilution the corresponding viscosity was 113- furol at 210 and afterdilution 375 Saybolt at"100 F. i

Example 10.0 lbs.'of a stock as used in the preceding Examples I, II orIII was diluted with a 70 viscosity (seconds Saybolt at 100 F.) mineralwhite oil to obtain a 30% mahogany sulfonate petroleum hydrocarbonsolution. To this was then added 1 lb. of sodium chlorite dissolved in2% lbs. of an aqueous sodium hypochlorite solution (about 10% availableClcontent). The mix was agitated and the temperature maintained at about180 to 200 F. The pH was adjusted to about 8. The treatment wasdiscontinued after a sample showed a reduced Lovibond color of about 2-3R (10% white oil cell). This result was achieved after about one-halfhour. The solution before treatment possessed a viscosity of about920seconds Saybolt at 100 F. andafter treatment with thechioritehypochlorite combination, a reduced viscosity of about 395seconds Saybolt at 100 F.

In the following table comparative viscosity data are furnishedofvarious sulfonate stocks showing in each case the viscosities of theun- -treated stock and of dilutions thereof to 30, and 40% sulfonatecontent, respectively, as against the viscosities of the same stock,treated with hypochlorite, chlorite or the chiorite-hypochloritecombination, respectively, and of 30, 35 and 40% sulfonate dilutions foreach treated stock. The respective treatments were carried out asspecified in Examples I, II or III. The'extending oil in each case was aneutral solvent refined mineral pale oil having a Saybolt viscosity of75 or seconds at 100 F. as specified.

Viscosity Reductions Obtained By Treatments as Shown Saybolt viscositiesat Na Hypochlorite alone in alk ph N a Chlorite alone in acid ph 100 F.When Ex- 7 Type of Sulionate Stock tended With vis.

Percent Furol neutral to Sodium Saybolt viscosities at Sayboltviscosities at Sodium Vis. at Sulfonate Content When Extended 100 WhenExtended Sulfonate 210 F. With 75 via. neutral With 75 vis. neutralFurol to Sodium Sulionate Furol to Sodium Sulfonate Vis. at Content Vis.at Content Av. M01 8 WL ource 30% 35% i 40% 30% 35% 40% 30% 35% 40% GulfCoast" 62 205 1,500 1,750 2,100 112 i 470 545 500 .108 475 545 590 Mid.001112.. 02 144 1,100 l, 280 1,475 74 395 490 570 72 400 492 576 Penna62 81 910 1,050 l, 200 38 375 470 560 40 375 472 562 CombinationChlorite-hypochlorite Type M summat smck j Saybolt viscosities at 100 F.When Ex- Saybolt viscosities at 100 F. When Extended With 75 vis.neutral to Sodium tended With 50 vis. neutral to Sodium Fugili vis. atSulionate Content Sulionate Content Av Mol. Wt Source 30% 35% 0% GulfCoast 475 550 590 Mid. Cont 73 400 495 675 Penna 39 380 475 560 240 28511 The following examples show various illustrations of the processingof textile materials in accordance with the invention.

Example V 820 lbs. of tailors clips were impregnated with a solution of'75 lbs. of a 30% petroleum sulfonate-mineral oil blend (prepared inaccordance with the procedure described in Examples I, II, III or IV) in300 lbs. of water heated to 160 F. The impregnation was accomplished byspraying the solution on the clips at the rate of about 4 gals, per 100lbs. of clips. The impregnated clips were allowed to remain overnight toinsure complete saturation and then run through a picker. The pickedstock was then blended with 18% cotton and again the blend run through amixing picker. The blend was then carded (there was no gumming on thecards) and spun into yarn. The yarn was then woven into fabric withcotton as the warp. The fabric was fulled without soap in water renderedslightly alkaline with about 2 oz. of soda ash per gallon of water.After failing, the fabric was scoured at 100 F. for about one-half hourwith plain water. There was copious sudsing and every indication of gooddetergency and dirt dispersion. Following the scouring, the fabric wasrinsed and dyed in the normal manner, no assistant being added to thedye: bath. The final fabric was superior in hand and general appearanceto the normal mill run in which in the scouring operation 4 oz. soda ashand 6 oz. soap per gallon were used, and with the scouring of whichadditionally equal quantities of alkali and soap were required.

Example VI 75 denier acetate yarn was impregnated with the solution ofpetroleum sulfonates used in Example V at 120 F. and secured out at 140F. with plain water. Analysis for matter extractible with ether showed90.2% scourability. Similar runs with 25% solution of petroleumsulfonates in oil gave a scourability of only 68.5% and after using soapand soda ash in amounts given in Example V as scouring assistants, ascourability of 77% .was determined.

Example VII A 25% emulsion of a 30% viscosity reduced mahogany'sulfonate solution, as is obtained for instance in accordance withExamples 1, II, III or IV, was prepared. This emulsion was then appliedat a temperature of about 130 F. to wool stock in the picker at a rateleaving on the wool about 24% (by weight of the wool) of the emulsion,i. e., an equivalent of about 6% of the sulfonate impregnant. Theemulsion was used in the form of a spray. The impregnated wool was thencarded, spun to yarn and woven into fabric. Prior to subjecting thefabric to a fulling operatiomthe same was soaked to drip-wetness withwater containing about 2% of soda ash and in this drip-wet condition wasthen subjected to fulling in the usual manner. Upon leaving the fullingmill, the lulled fabric was subjected to a scouring operation byrepeatedly washing the same with plain water (i. e., without addition ofscouring agent) having a temperature of approximately 105 to 110 F.until substantially all of the impregnant and other impurities wereremoved. As compared with the amounts of scour-. ing water required forwool goods carrying conventional impregnants, the fulled materialobtained in this case required considerab y E55 12 scouring water andthe time of scouring and rinsing treatment was reduced to about half ofthat normally required by goods impregnated with conventional typeimpregnants. After scouring, extraction tests showed removal ofimpregnant to an extent of about 96%.

Example VIII Wool goods impregnated and processed as described inExample VII and as they come from the fulling mill were subjected to arinse in the dyeing .machine with weakly ammoniacal water and afterremoval of the aqueous rinsing medium were dyed in the normal manner.After dyeing extraction tests showed removal of impregnant in the dyebath to an extent of I Example IX A 1% aqueous emulsion was preparedusing a 30% viscosity reduced (185 seconds Saybolt at 100 F.) mahoganysulfonate lubricant solution as for instance obtained by subjecting a420 Pennsylvania sulfonate stock to the procedures set forth in ExamplesI, II or In and extending with a 50 vis. neutral (see table, lastcolumn). Viscose filament cakes were contacted with this emulsion for atime sufiicient to leave on or in the filaments, after removal of excessemulsion, about /2 to 74% (by dry weight of the filament) of thesulfonate lubricant. The emulsion soaked filament cakes were thencentrifuged for removal of excess emulsion and the filaments dried andconed. The coned filaments were then warped" and thereafter sized withthe application of a size solution containing about 4% gelatin but nowetting agent. After treatment, about 2% of size is left on the warpwhereupon the goods were woven into fabric and the fabric subjected to aboil-oil operation by immersing the same in weakly ammoniacal hot waterof about to F. No scouring or boil-off agent was used in the boil-oil.The goods were then subjected to a dyeing operation in the usual manner.The goods exhibited level dyeing. Extraction tests of the boiled oilgoods showed removal of impregnant to an extent of about 95%.

The percentage impregnant removedon scouring or boll-ofl' shown inExamples V-IX was ascertained in the usual manner by soxhlet etherextraction. The extracted material showed the residue left on the fibreafter scouring or boil-off, thus indicating the amount of impregnantactually removed by that operation.

Instead of using for the wool or synthetic fibre impregnation asspecified in Examples V to IX any of the viscosity reduced impregnantsobtained in accordance with Examples I, II, III or IV. any othersuitable viscosity reduced mahogany sulfonate hydrocarbon solution maybe used as may be for instance obtained by other viscosity reducingtreatment such aswith Ch, C102, 'dimethyl phthalate or any othersimilarly reacting material.

The extent to which low viscosity values may be obtained depends, atleast to some extent, upon the type or origin of the petroleum mahoganysuifonate selected for the treatment. Ordinarily high average molecularweight sulfonates possess a higher viscosity and the resulting viscosityafter treatment is usually commensurately higher than the viscosityafter treatment of a comparative sulfonate hydrocarbon solution whichbefore treatment possessed a relatively lower viscosity and in which thesulfonate had a lesser average molecular weight.

The foregoing description is for purposes of illustration and not oflimitation and it is therefore my intention that the invention belimited only .by the appended claims or their equivalents wherein I haveendeavored to claim broadly all inherent novelty.

I claim:

1. A textile treating agent which comprises a hydrocarbon textilelubricating oil and substantially dissolved therein at least 28% alkalimetal petroleum mahogany sulfonate obtained by reacting a petroleummahogany sulfonatesolution in an organic substantially water immisciblesolvent for said sulfonate, with an oxidation agent selected from thegroup consisting of oxidation agents having an oxidation potential insuch solution by reason of available 02 and those having an oxidationpotential in such solution by reason of available C12 in amount and fora period of time sufficient to yield for its said at least 28% sulfonatesolution a Saybolt viscosity at 100 F. of not in excess of 600 seconds.

2. A textile treating'agent in accordance with claim 1 in which saidhydrocarbon textile lubricating oil contains dissolved therein from 28to of the said oxidation agent reacted petroleum mahogany sulfonate.

3. A textile treating agent in accordance with claim 2 in which saidalkali metal petroleum mahogany sulfonate is one obtained by reactionwith said oxidation agent in amount and for a period of time sufficientto impart to its said hydrocarbon textile lubricating oil solution aSaybolt viscosity at 100 F. of not in excess of 300 seconds.

4. A textile treating agent which comprises a hydrocarbon textilelubricating oil and substantially dissolved therein from 28 to 40%alkali metal petroleum mahogany sulfonate obtained by reacting apetroleum mahogany sulfonate solution in an organic substantially waterimmiscible solvent for said sulfonate, with an oxidation agent having anoxidation potential in said. solution by reason of available Oz inamount and for a period of time sufficient to yield for its said atleast 28 to 40% sulfonate solution a Saybolt viscosity at 100 F. of notin excess of 600 seconds.

5. A textile treating agent which comprises a hydrocarbon textilelubricating oil and substantially dissolve therein from 28 to 40% alkalimetal petroleum mahogany sulfonate obtained by reacting a petroleummahogany sulfonate solution in an organic substantially water immisciblesolvent for said suifonate, with an oxidation agent having an oxidationpotential in said solution by reason of available" C12 in amount and fora period of time sufficient to yield for its said at least 28 to 40%sulfonate solution a Saybolt viscosity of 100 F. of not in excess of 600seconds.

6. A substantially self-scouring lubricated textile material whichcomprises a textile material impregnated with a viscosity reducedpetroleum mahogany sulfonate solution consisting of a hydrocarbontextile lubricating oil and substantially dissolved therein at least 28%alkali metal petroleum mahogany sulfonate obtained by reacting'apetroleum mahogany sulfonate solution in an organic substantially waterimmiscible solvent for said sulfonate, with an oxidation agent selectedfrom the group consisting of oxidation agents having an oxidationpotential in such solution by reason of available 02 and those having anoxidation potential in such solution by reason of available C12 inamount and for a period of time sufiicient to yield for its said atleast 28% sulfonate solution a Saybolt viscoslty at 100 F. of not inexcess of 600seconds.

ABRAHAM MOSCOWITZ.

REFERENCES CITED Bio of this patent:

UNITED STATES PATENTS Blumer Mar. 19, 1946

